CN109607557A - A kind of high-purity titanium diboride raw powder's production technology - Google Patents
A kind of high-purity titanium diboride raw powder's production technology Download PDFInfo
- Publication number
- CN109607557A CN109607557A CN201910122617.3A CN201910122617A CN109607557A CN 109607557 A CN109607557 A CN 109607557A CN 201910122617 A CN201910122617 A CN 201910122617A CN 109607557 A CN109607557 A CN 109607557A
- Authority
- CN
- China
- Prior art keywords
- powder
- titanium diboride
- production technology
- purity
- purity titanium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
- C01B35/04—Metal borides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of high-purity titanium diboride raw powder's production technologies, are related to boride powder preparation field, are to solve existing TiB2The problems such as preparation process is at high cost, complex process.Specific step is as follows: step 1 by the present invention, by B4C powder, TiO2Powder and carbon black powder mixing 10-30min, obtain the first mixture；Step 2 the first mixture is added in the sintering furnace of inert atmosphere, and sintering furnace is warming up to 1500-1700 DEG C and keeps 3-4h, and finished product is obtained after natural cooling.The present invention selects the process conditions such as suitable raw material proportioning, firing temperature, finally obtains high-purity Ti B2Powder has many advantages, such as that simple process, purity is high, firing temperature are low, granularity is small, at low cost, easy industrialized production, has broad application prospects.
Description
Technical field
The present invention relates to boride powder preparation field, specifically a kind of high-purity titanium diboride raw powder's production technology.
Background technique
TiB2It is compound uniquely stable in Ti-B binary system, as a kind of very important ceramic material, TiB2Have
High-melting-point (3225 DEG C), ultrahigh hardness (HV=34GPa) and intensity, excellent conductive, thermally conductive, antioxygenic property, chemical stabilization
The advantages that property is good.TiB2It can be soaked by molten metal, TiB2 is used in modern aluminium electrolytic industryYinPole can reduce aluminium electroloysis
Power consumption.TiB2Since its good conductivity and resist melt non-ferrous metal metal erosion ability be used to make high temperature and lead
Electric evaporation boat.TiB2As the important component of multi-element composite material, with ZrB2、ZrC、SiC、Al2O3Equal ceramic materials are multiple
It closes, improves its electric conductivity, machining property, mechanical characteristic etc., in rocket nozzle, aero engine turbine blades, cutting tool
Have broad application prospects with the fields such as wear parts, surface covering and plated film and nuclear industry material.
At present about TiB2Preparation process and synthesis report it is existing very much.Chinese patent CN105884371A discloses one
Kind submicron order TiB2The self-propagating synthesis method of powder: a certain proportion of TiO that will be mixed2、B2O3, metal magnesium powder is put into
It is placed in the indoor graphite boat of self-propagating reaction, heating causes self-propagating reaction, through pickling impurity removal, washing, drying and grinds
The TiO for being 98.5% to purity2Powder.The TiB of this method preparation2Purity is high, but technique is cumbersome, needs multiple pickling, washed with impurities,
High production cost, industrialized production are difficult.Chinese patent document CN106631032A discloses a kind of high-purity titanium diboride powder
And preparation method thereof: by a certain proportion of B4C、TiO2, carbon black mixed in batch mixer, be directly placed into intermediate-frequency heating furnace
It is burnt into 30-40h at 2000-2200 DEG C, obtains the TiB that purity is 99.5%2Powder.The TiB2 powder purity of this method preparation
Height, but the firing temperature of technique is high, and the reaction time is long, at high cost.Chinese patent document CN101704674A discloses one kind certainly
The method that sprawling high―temperature nuclei prepares titanium biboride ceramic micropowder: by granularity less than 100 mesh, purity is greater than 99% titanium valve and boron
Powder is mixed in a certain proportion rear cold moudling, ignites in vacuum indoor electric arc, broken combustion product obtains 2-8 μm of TiB2Pottery
Porcelain micro mist.The TiB of this method preparation2Powder granularity is uniform, but it is at high cost, industrialized production is difficult.
Summary of the invention
The purpose of the present invention is to provide a kind of high-purity titanium diboride raw powder's production technologies, to solve above-mentioned background technique
The problem of middle proposition.
To achieve the above object, the invention provides the following technical scheme:
A kind of high-purity titanium diboride raw powder's production technology, the specific steps are as follows:
Step 1, by B4C powder, TiO2Powder and carbon black powder mixing 10-30min, obtain the first mixture；
Step 2, by the first mixture be added inert atmosphere sintering furnace in, sintering furnace be warming up to 1500-1700 DEG C and
3-4h is kept, obtains finished product after natural cooling.
As a further solution of the present invention: B4The quality of C powder is B4C powder, TiO2Powder and carbon black powder gross mass
20-40%, the quality of carbon black powder is B4C powder, TiO2The 15-20% of powder and carbon black powder gross mass.
As a further solution of the present invention: B4The partial size of C powder is 1.5-7.5 μm, and purity is 99.6% or more, TiO2
Powder is anatase thpe white powder, and partial size is 0.3-1 μm, and purity 99.5%, the partial size of carbon black powder is 0.5-1 μm.
As a further solution of the present invention: B in step 14C powder, TiO2Powder and carbon black powder are 800- in revolving speed
It is mixed in the fly cutter batch mixer of 1000r/min.
As a further solution of the present invention: the heating rate of sintering furnace is 5-10 DEG C/min in step 2.
As a further solution of the present invention: the first mixture is added in sintering furnace by graphite boat, and easy fired is cooling
Afterwards without grinding the high-purity Ti B up to 4-7 μm of granularity2Powder.
As a further solution of the present invention: fly cutter batch mixer is made of stainless steel material, and material is easy to get, using effect
It is good, long service life.
As a further solution of the present invention: insertion slot type cover board in hole is had on graphite boat, it is possible to reduce the volatilization of boron element,
Crystallization body pollution is reduced simultaneously.
The present invention completes TiB using carbothermic method in carbon shirt-circuiting furnace2The synthesis of powder, specific reaction equation are as follows: B4C+
2TiO2+3C→2TiB2+4CO↑。
Compared with prior art, the beneficial effects of the present invention are:
The present invention selects the process conditions such as suitable raw material proportioning, firing temperature, finally obtains high-purity Ti B2Powder has
The advantages that simple process, purity is high, firing temperature are low, granularity is small, at low cost, easy industrialized production, before wide application
Scape.
Detailed description of the invention
Fig. 1 is the flow chart of high-purity titanium diboride raw powder's production technology.
Fig. 2 is that the XRD of 1 product of embodiment in high-purity titanium diboride raw powder's production technology detects figure.
Fig. 3 is that the XRD of 2 product of embodiment in high-purity titanium diboride raw powder's production technology detects figure.
Fig. 4 is that the XRD of 3 product of embodiment in high-purity titanium diboride raw powder's production technology detects figure.
Fig. 5 is that the XRD of 1 product of comparative example in high-purity titanium diboride raw powder's production technology detects figure.
Specific embodiment
The technical solution of the patent is explained in further detail With reference to embodiment.
Embodiment 1
The present embodiment provides a kind of high-purity Ti B2Powder and its low temperature preparation method, as shown in Figure 1, including the following steps:
1) by B4C powder 6.9Kg, granularity are 6 μm, purity 99.6%, TiO2Powder 18.9Kg, granularity are 0.5 μm, and purity is
99.5%, carbon black powder 4Kg, granularity are 1 μm, are put into fly cutter batch mixer and mix 30min, and fly cutter revolving speed is 880r/min；
2) 1) mixed uniformly raw material in is put into graphite boat, boat sintering is pushed away in carbon shirt-circuiting furnace, pushes away boat time 3h, carbon shirt-circuiting furnace
Heating rate be 8 DEG C/min, sintering temperature be 1700 DEG C；
3) TiB for being 99.6% up to purity is crushed after natural cooling2Powder, diameter of particle is 4.6 μm after being crushed.
Embodiment 2
The present embodiment provides a kind of high-purity Ti B2Powder and its low temperature preparation method, include the following steps:
1, by B4C powder 6.9Kg, granularity are 2 μm, purity 99.6%, TiO2Powder 18.9Kg, granularity are 0.3 μm, and purity is
99.5%, carbon black powder 4Kg, granularity are 0.5 μm, yttrium oxide 0.15Kg, and granularity is 15-25 μm, are put into fly cutter batch mixer and mix
30min, fly cutter revolving speed are 1000r/min；
2,1) mixed uniformly raw material in is put into graphite boat, boat sintering is pushed away in carbon shirt-circuiting furnace, pushes away boat time 3h, carbon shirt-circuiting furnace
Heating rate be 5 DEG C/min, sintering temperature be 1500 DEG C；
3) TiB for being 99.2% up to purity is crushed after natural cooling2Powder, diameter of particle is 6.4 μm after being crushed.
Embodiment 3
The present embodiment provides a kind of high-purity Ti B2Powder and its low temperature preparation method, include the following steps:
1) by B4C powder 7.2Kg, granularity are 2 μm, purity 99.6%, TiO2Powder 18.9Kg, granularity are 0.3 μm, and purity is
99.5%, carbon black powder 4.2Kg, granularity are 0.5 μm, are put into fly cutter batch mixer and mix 30min, and fly cutter revolving speed is 1000r/min；
2) 1) mixed uniformly raw material in is put into graphite boat, boat sintering is pushed away in carbon shirt-circuiting furnace, pushes away boat time 4h, carbon shirt-circuiting furnace
Heating rate be 10 DEG C/min, sintering temperature be 1600 DEG C；
3) TiB for being 99.4% up to purity is crushed after natural cooling2Powder, diameter of particle is 5.9 μm after being crushed.
Comparative example 1
The present embodiment provides a kind of high-purity Ti B2 powder and its low temperature preparing methods, include the following steps:
1) by B4C powder 6.9Kg, granularity are 15 μm, purity 99.6%, TiO2Powder 18.9Kg, granularity are 1 μm, and purity is
99.5%, carbon black powder 4Kg, granularity are 5 μm, are put into fly cutter batch mixer and mix 30min, and fly cutter revolving speed is 600r/min；
2) 1) mixed uniformly raw material in is put into graphite boat, boat sintering is pushed away in carbon shirt-circuiting furnace, pushes away boat time 3h, carbon shirt-circuiting furnace
Heating rate be 8 DEG C/min, sintering temperature be 1400 DEG C；
3) TiB for being 96.82% up to purity is crushed after natural cooling2Powder, 10.6 μm of diameter of particle after being crushed.
The product to embodiment 1-3 and the product of comparative example 1 carry out analysis of chemical elements and XRD detection, chemistry member respectively
The result that the results are shown in Table 1, XRD detection of element analysis is shown in Fig. 2-5.
Table 1
| B | Ti | C | O | Fe | |
| Embodiment 1 | 30.99 | 68.61 | 0.084 | 0.3 | 0.016 |
| Embodiment 2 | 30.9 | 68.3 | 0.21 | 0.57 | 0.02 |
| Embodiment 3 | 30.93 | 68.47 | 0.12 | 0.462 | 0.018 |
| Comparative example 1 | 30.53 | 66.29 | 0.1 | 2.826 | 0.024 |
The result of XRD detection and the result of analysis of chemical elements are it is found that the product of comparative example 1 is compared in 1400 DEG C of sintering
It is reduced in embodiment 1-3 sintering temperature, raw material fails to react completely, while reducing the additional amount of boron element, the purity of product
It reduces.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.No
It should treat any reference in the claims as limiting the claims involved.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (8)
1. a kind of high-purity titanium diboride raw powder's production technology, which is characterized in that specific step is as follows:
Step 1, by B4C powder, TiO2Powder and carbon black powder mixing 10-30min, obtain the first mixture；
Step 2 the first mixture is added in the sintering furnace of inert atmosphere, and sintering furnace is warming up to 1500-1700 DEG C and keeps
3-4h obtains finished product after natural cooling.
2. high-purity titanium diboride raw powder's production technology according to claim 1, which is characterized in that the B4The matter of C powder
Amount is B4C powder, TiO2The 20-40% of powder and carbon black powder gross mass, the quality of carbon black powder are B4C powder, TiO2Powder
With the 15-20% of carbon black powder gross mass.
3. high-purity titanium diboride raw powder's production technology according to claim 1, which is characterized in that the B4The grain of C powder
Diameter is 1.5-7.5 μm, TiO2Powder is anatase thpe white powder, and partial size is 0.3-1 μm, and the partial size of carbon black powder is 0.5-1 μm.
4. high-purity titanium diboride raw powder's production technology according to claim 1, which is characterized in that B in the step 14C
Powder, TiO2Powder and carbon black powder mix in the fly cutter batch mixer that revolving speed is 800-1000r/min.
5. high-purity titanium diboride raw powder's production technology according to claim 1, which is characterized in that burnt in the step 2
The heating rate of freezing of a furnace is 5-10 DEG C/min.
6. high-purity titanium diboride raw powder's production technology according to claim 1, which is characterized in that first mixture
It is added in sintering furnace by graphite boat.
7. high-purity titanium diboride raw powder's production technology according to claim 4, which is characterized in that the fly cutter batch mixer
It is made of stainless steel material.
8. high-purity titanium diboride raw powder's production technology according to claim 6, which is characterized in that band on the graphite boat
There is hole insertion slot type cover board.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910122617.3A CN109607557A (en) | 2019-02-18 | 2019-02-18 | A kind of high-purity titanium diboride raw powder's production technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910122617.3A CN109607557A (en) | 2019-02-18 | 2019-02-18 | A kind of high-purity titanium diboride raw powder's production technology |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109607557A true CN109607557A (en) | 2019-04-12 |
Family
ID=66019059
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910122617.3A Pending CN109607557A (en) | 2019-02-18 | 2019-02-18 | A kind of high-purity titanium diboride raw powder's production technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109607557A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111470868A (en) * | 2020-03-30 | 2020-07-31 | 江苏大学 | High-activity submicron boron carbide ceramic powder and low-temperature in-situ preparation method thereof |
| CN114132959A (en) * | 2021-11-15 | 2022-03-04 | 武汉科技大学 | Core-shell structure B4C@TiO2Composite powder and preparation method thereof |
| CN114394834A (en) * | 2022-02-22 | 2022-04-26 | 中硼科技(威海)有限公司 | Preparation method of boron carbide-based nano composite powder |
| WO2023057716A1 (en) * | 2021-10-04 | 2023-04-13 | Saint-Gobain Centre De Recherche Et D'etudes Europeen | Process for synthesising a titanium diboride powder |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5100845A (en) * | 1991-03-13 | 1992-03-31 | Union Carbide Coatings Service Technology Corporation | Process for producing titanium diboride and boron nitride powders |
| CN101704674A (en) * | 2009-11-11 | 2010-05-12 | 昆明理工大学 | Method for preparing titanium diboride ceramic micro powder by self-propagation high temperature synthesis |
| CN101891215A (en) * | 2010-07-15 | 2010-11-24 | 武汉工程大学 | Method for preparing nano titanium diboride polycrystalline powder |
| CN104944432A (en) * | 2015-06-30 | 2015-09-30 | 莱芜亚赛陶瓷技术有限公司 | Superfine 10B-rich titanium diboride powder and preparation method thereof |
| CN106631032A (en) * | 2016-10-12 | 2017-05-10 | 淄博晶亿陶瓷科技有限公司 | High-purity titanium diboride powder and preparation method thereof |
-
2019
- 2019-02-18 CN CN201910122617.3A patent/CN109607557A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5100845A (en) * | 1991-03-13 | 1992-03-31 | Union Carbide Coatings Service Technology Corporation | Process for producing titanium diboride and boron nitride powders |
| CN101704674A (en) * | 2009-11-11 | 2010-05-12 | 昆明理工大学 | Method for preparing titanium diboride ceramic micro powder by self-propagation high temperature synthesis |
| CN101891215A (en) * | 2010-07-15 | 2010-11-24 | 武汉工程大学 | Method for preparing nano titanium diboride polycrystalline powder |
| CN104944432A (en) * | 2015-06-30 | 2015-09-30 | 莱芜亚赛陶瓷技术有限公司 | Superfine 10B-rich titanium diboride powder and preparation method thereof |
| CN106631032A (en) * | 2016-10-12 | 2017-05-10 | 淄博晶亿陶瓷科技有限公司 | High-purity titanium diboride powder and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111470868A (en) * | 2020-03-30 | 2020-07-31 | 江苏大学 | High-activity submicron boron carbide ceramic powder and low-temperature in-situ preparation method thereof |
| WO2023057716A1 (en) * | 2021-10-04 | 2023-04-13 | Saint-Gobain Centre De Recherche Et D'etudes Europeen | Process for synthesising a titanium diboride powder |
| CN114132959A (en) * | 2021-11-15 | 2022-03-04 | 武汉科技大学 | Core-shell structure B4C@TiO2Composite powder and preparation method thereof |
| CN114132959B (en) * | 2021-11-15 | 2024-04-02 | 武汉科技大学 | Core-shell structure B 4 C@TiO 2 Composite powder and preparation method thereof |
| CN114394834A (en) * | 2022-02-22 | 2022-04-26 | 中硼科技(威海)有限公司 | Preparation method of boron carbide-based nano composite powder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109607557A (en) | A kind of high-purity titanium diboride raw powder's production technology | |
| CN109180188B (en) | High-entropy boron-containing carbide ultra-high temperature ceramic powder and preparation method thereof | |
| CN108101533B (en) | Preparation method of ceramic target material for thermal barrier coating | |
| CN110511035A (en) | A kind of high entropy ceramics of high-ductility high wear-resistant and its preparation method and application | |
| CN108455614B (en) | Method for preparing nano WC powder at low temperature and in short process | |
| CN105272260B (en) | A kind of soap-free emulsion polymeization phase tungsten carbide composite and preparation method thereof | |
| US20090105062A1 (en) | Sintered Wear-Resistant Boride Material, Sinterable Powder Mixture, for Producing Said Material, Method for Producing the Material and Use Thereof | |
| CN103754891B (en) | The method of a kind of boron/carbothermic method low-temperature growth hafnium boride powder | |
| CN103408015B (en) | Preparation method of ultrafine tungsten carbide powder | |
| CN110407213B (en) | (Ta, nb, ti, V) C high-entropy carbide nano powder and preparation method thereof | |
| CN104387073B (en) | The method of ultra-fine high tenacity thyrite is manufactured based on reaction sintering | |
| CN106631033A (en) | Method for preparing ZrB2 powder | |
| CN107904472A (en) | A kind of manufacture method of non-magnetic alloy | |
| CN106631032B (en) | A kind of high-purity titanium diboride powder and preparation method thereof | |
| CN112125686A (en) | Method for preparing silicon carbide coated graphite by molten salt isolation | |
| CN1699168A (en) | Combustion synthesis method of zirconium diboride micro-powder | |
| CN109608191B (en) | A kind of high intensity gray oxide zircon ceramic and preparation method thereof | |
| CN103979567B (en) | A kind of low-temperature growth CrB or CrB 2the method of powder | |
| CN101519746A (en) | Molybdenum-base compound material and preparation method thereof | |
| CN108251670A (en) | The preparation method of compound alloy between refractory metal | |
| CN109665848A (en) | A kind of superhigh temperature SiC-HfB2Composite ceramics and its preparation method and application | |
| CN114959287B (en) | Rare earth metal or rare earth alloy purification material, preparation method thereof and rare earth metal or rare earth alloy purification method | |
| CN109704802A (en) | One kind ceramic modified C/C composite material and preparation method of (Zr, Hf) B-SiC | |
| CN115072732A (en) | Preparation method of titanium diboride ultrafine powder | |
| CN108622911B (en) | Superfine zirconium diboride-silicon carbide composite powder and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190412 |
|
| RJ01 | Rejection of invention patent application after publication |